Dimethylamine → HCID 4467695、化合物

HRID 1446154ノート

反応式

HRID 1446154 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:12]([C:13](O)=[O:14])=[C:11]([CH3:16])[O:10][N:9]=1.S(Cl)(Cl)=O.[CH3:21][NH:22][CH3:23]>>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:12]([C:13]([N:22]([CH3:23])[CH3:21])=[O:14])=[C:11]([CH3:16])[O:10][N:9]=1

参加物

4

反応物 3

HCID 674DimethylamineHCID 24386Thionyl ChlorideHCID 902034-Isoxazolecarboxylic acid, 3-(2-chlorophenyl)-5-methyl-

生成物 1

HCID 4467695HCID 4467695、化合物収率 23.6%

反応条件

温度
60 °C

実験手順

To 3-(2-chlorophenyl)-5-methylisoxazol-4-carboxylic acid (25 mg, 0.10 mmol) was added thionyl chloride (1 mL) and the neat solution allowed to stir 60° C. After 30 min, excess thionyl chloride was evaporated and dimethyl amine (40 μL, 0.08 mmol, 2M in tetrahydrofuran) was added and allowed to stir overnight at ambient temperature. The residue was purified using reversed phase HPLC to afford the title compound (5 mg). HRMS (ESI, pos. ion) m/z calcd for C13H13ClN2O2: 264.0666, found 264.0669.

後処理

  1. customexcess thionyl chloride was evaporated
  2. stirringto stir overnight at ambient temperature
  3. customThe residue was purified

出典と根拠

ORDレコード
ord-0d5037ad7476428a856729169b98b565
出典データセット
uspto-grants-2010_02
特許番号
US07666888B2

反応ノート

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